Production and utilization of sulfonated stearic products.



IVAN LEvINs'rnIiv,

PRODUCTION UTILIZATION OF SULFONATED STEABIO PR ODUCTS.

No Drawing.

To all whom it may concern:

Be it known that I, IVAN Lrvnvs'rnrn, a' subject of .the King of Great Britain and Ireland, and a resident of Manchester, in

the county of Lancaster, England, have invented new and useful Improvements mand Relating to the Production and Util zation of Sulfonated Stearic Products, of which the-following is a specification.

Lewkovitch, Chemical Technology of Oils, Fats and vl Vrrres, vol. '3, page 181, (1909 edition) refers to sulfonated compounds .of fats, but the method given is of fats, nor was it intended to be.

not a practicable one for'the sulfonatiIoIn e H states on the same page that. the behavior of the sulfuricacid to the stearic glycerids is of little practical importance since any sulfonated compounds that are formed are subsequently decomposed,yield- 'ng the original stearic acid practically unchanged. In confirmation of this quotatron from Lewkovitch, a large number of experiments I-have made have shown that pure stearic acid does not yield stearic sulfo' compounds, .at least not by any hitherto known method of sulfonating oils. In experiments I have not only applied the usual methods but have varied the procedure with regardato temperature, strength of sulfuric acid,-duration of reaction and the like, but I have always obtained negative results, that is the stearic acid has remained unchanged. I have found however that stearic acid which has been combined with oi mixed with a fat, oil, orthe like capable of forming sulfon'ated coinpounds will, when treated in such mixture or compound in the manner hereinafter described, yield 'ste iric sulfo acids. The cgm ru'rent production of "tassel-f0 compounds ofthe stearic acid and of the fat, oil, grease or the like which is combined or mixed with the stearic acid renders the sulfostearic compound a permanent one which may be used in the treatment of leather during itspreparation, and also in thefinishing of textile ing facts.

ing compounds with fats, semi-fats, greases Specification of Letters Patent. Patented 11 21 1916 Application filed February 1'7, 1914. Serial No. 819,169. I

or waxes which compounds are soluble or emulsifiable. or miscible in or-With water. See for example my prior British patent specification No. 18333 of 1912. vThe sulfo na ted compounds produced according to this invention possess this same remarkable UNITED STATES 11mm; OFFICE; f

or MANCHESTER, ENGLAND, nssrenon r0 COMPANY or LEVIN- STEIN LIMITED, or MANCHESTER, ENGLAND. l

property ,of rendering fats, waxes or the like soluble or miscible or niiilsifiable even when the fat or oil'which' is concurrently sulfonated with the stearic acid yields sulfo compounds which will not render the fats, Waxes, or the like soluble or miscible in water. The property, then, which compounds produced according to this invention do possess of rendering fats, waxes, or the like permanently soluble or'miscible must reside in the sulfo stearic acid produced.

This invention consists (a) in sulfonating the stearic acidconcurrently with a suitable fat, oil or the like and (b) in the pro -andgreases, fats, waxes or the like.-

A generally convenient mode of operation to produce the v desired permanent sulfo "'stearic acid is to melt the substance which contains the ste'aric'acid, and then to cool it' down until-it is about 5 C. lower in temperature than the temperature at which the sulfonation is to be carried out. Then add duction of miscible soluble or, emulsifiable compounds of the joint sulfonated products gradually sulfuric acid (for preference 100% H SO, monohydrate) and continue at the stated temperature until sulfonation is complete, that is until a sample taken from the sulfonation melt is miscible with hot water.

tion, the s'ulfonationmelt into a 10% salt;

solution which has previously been heated 1 :to 30-35 (l, Stopagitation and allow the mass to settle,.- keeping 'thetemperature of the salt solution between 30-35 G., and as soon as the oil or grease or fat has .se'pa-:

rated run ofl' the warm salt solution. The oil or fat remaining is then melted up again and allowed to settle to further remove mineral acid, or the latter may be neutraliZcd or partially neutralized with an alkali. The resulting sulfonation compound, if the mineral acid has all been removed, is the free sulfo acid which is of a suitable char-" acter. Care has to be taken that the finishing process is carried out as quickly as possible as these compounds are very liable to hydrolize during this stage.

Then pour," under constantagita- Lwl The following are examples of Substances, proportions, temperatures and the'like employed in carrying this invention into effect.

Example 1: 200 parts of commercial stearin (melting point 45 C.) are melted and then cooled to 40 C. stirring all the while. Commercial stearin contains a considerable portion of free fat and the use of this product may be regarded equivalent to the use of stearin itself with a fat added thereto. 50 parts of sulfuric acid monohydrate are slowly added and the temperature kept between .l5 and 50 C. until a sample of the melt is miscible in hot Water. The finishing process is as stated above.

Example 2: 200 parts of pure stearic acid are melted together with 200 parts of distilled wool stearin, cooled to about 40 C. and sulfonatcd as above described at a temperature-of from 40 to 50 C.

' Example 3: 200 parts of pure stearic acid are melted with 200 parts of wool grease.

The method is the same as that given in Example 1 except that during sulfonation the temperature is kept between 35 and 40 C. \Vool stearin is a waxy substance consisting mainly of cholesterols obtained from the wool greases of'bnimerce. It is frequently referred to as anhydrous lanolin or as wool Wax or wool fat.

The wool grease, referred to in Example 3,

Example 200 parts of commercial stearin are melted with 200 parts of tallow. Temperature of sulfonation 40 C.

Example 7; 200 parts of distilled 6601 stearin are melted with 200 parts of'wool grease. Temperature of sulfonation 35 to 40 C. v 7 Example 8: Equal parts. of commercial stearin and palm oil are melted together and cooled to 40 C. To 200 parts of this mixture 50 parts of 100% I-LSO are gradually added. Sulfonation temperature 10 to 45 C.

. Example 9: Equal parts of commercial stearin and Japan wax are melted together and cooled to 35 C. Sulfonated as in preceding example but at a'temperature' of The sulfo compounds of stea ric acid produced as above described may be melted andmixed with other fats, oils, waxe's s iich as paraliin'wax', or greases such as tallow, to render such fats, oils, or the like soluble or emulsifiable in or miscible with water.

. In the above examples the stearic acid'or the source of stearic acid has only been described as being melted and. mixed with a single oil, fat or the like for sulfonation, but if desired it may be melted and mixed with two or more oils or the like for sulfonation.

In the claims the generic term fat will be used and intended to cover either. a-solid .fat, fatty 'oil,fgrease or the like, which is concurrently treated with sulfuric acid with the stearic acid, or is thereafter mixed with the sulfonated compound thus formed to provide the miscible compound whichforms the desired product; and it is intended also that the term miscible be suliiciently' broad to cover any miscible, soluble or emulsifiable compound of the character described; the term wax as hereinafter used, is regarded sufiicientlybroad to cover such compounds as are generally covered by thds term in the standard authorities.

What I claim is 1. The production of a permanent sulfo stearic compound by concurrently treating with sulfuric acid, stearic acid and a fat capable of formmg a sulfo compound, substantially as hereinbefore described.

2. A sulfonated compound containing a permanent sulfo stearic compound and a sulfo compound of a 'fat, substantially as described.

3. The production of a miscible compound I of a fat or wax by admixture of the fat or wax with a sulfonated compound containing a permanent sulfo stearic compound and a sulfo compound of a fat, substantially as set forth,

4. A.misc1ble compound containing a fat or wax, aj sulfo compound of stearic a'cid and a sulfo compound of a fat, substantially as set forth. r I a In witness whereof I have hereunto set my hand in the presence of two subscribing witnesses.

Witnesses: VILLIAM Gno. HEYL, GEORGE WEAVER.

IVAN Lnvlustrnru. 

